JP5614689B2 - 水酸化コバルト(ii)・鉄(iii)六角板状層状結晶の製造方法 - Google Patents
水酸化コバルト(ii)・鉄(iii)六角板状層状結晶の製造方法 Download PDFInfo
- Publication number
- JP5614689B2 JP5614689B2 JP2012005050A JP2012005050A JP5614689B2 JP 5614689 B2 JP5614689 B2 JP 5614689B2 JP 2012005050 A JP2012005050 A JP 2012005050A JP 2012005050 A JP2012005050 A JP 2012005050A JP 5614689 B2 JP5614689 B2 JP 5614689B2
- Authority
- JP
- Japan
- Prior art keywords
- iron
- hexagonal plate
- iii
- cobalt hydroxide
- layered
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000013078 crystal Substances 0.000 title claims description 83
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 title claims description 65
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 title claims description 59
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 title claims description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- -1 iodine anions Chemical class 0.000 claims description 30
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 26
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 26
- 239000011630 iodine Substances 0.000 claims description 22
- 229910052740 iodine Inorganic materials 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 13
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 13
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 12
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- PKSIZOUDEUREFF-UHFFFAOYSA-N cobalt;dihydrate Chemical compound O.O.[Co] PKSIZOUDEUREFF-UHFFFAOYSA-N 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 4
- 229960002089 ferrous chloride Drugs 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 3
- KJIYBINEQTYQCF-UHFFFAOYSA-N cobalt;hexahydrate Chemical compound O.O.O.O.O.O.[Co] KJIYBINEQTYQCF-UHFFFAOYSA-N 0.000 claims description 3
- 150000004685 tetrahydrates Chemical class 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 239000010410 layer Substances 0.000 description 16
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 15
- 239000002135 nanosheet Substances 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- 239000002356 single layer Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 238000001000 micrograph Methods 0.000 description 10
- 239000007787 solid Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 5
- 238000002411 thermogravimetry Methods 0.000 description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- BAZAXWOYCMUHIX-UHFFFAOYSA-M sodium perchlorate Chemical compound [Na+].[O-]Cl(=O)(=O)=O BAZAXWOYCMUHIX-UHFFFAOYSA-M 0.000 description 4
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000005349 anion exchange Methods 0.000 description 3
- 229910052599 brucite Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229910020366 ClO 4 Inorganic materials 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000642 polymer Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical class [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- IXGNPUSUVRTQGW-UHFFFAOYSA-M sodium;perchlorate;hydrate Chemical compound O.[Na+].[O-]Cl(=O)(=O)=O IXGNPUSUVRTQGW-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Description
ここで、前記処理するステップは、ヨウ素及び水のクロロホルム溶液中に水酸化コバルト(II)・鉄(II)六角板状層状結晶を分散させ、室温で攪拌するステップであってよい。
また、前記水酸化コバルト(II)・鉄(II)六角板状層状結晶はブルーサイト型結晶であってよい。
また、前記水酸化コバルト(II)・鉄(II)六角板状層状結晶は厚さが1×102nm〜5×102nmであってよい。
また、前記水酸化コバルト(II)・鉄(II)六角板状層状結晶は、塩化コバルト・六水和物と塩化第一鉄・四水和物との混合物の水溶液に窒素ガスを流すと共にヘキサメチレンテトラミンを加えた後、還流させることにより製造してよい。
次に、実施例を示して、さらに具体的に説明する。
マグネティックスタラーおよび窒素導入管を取り付けた1000cm3の三口フラスコに、和光純薬工業(株)製の塩化コバルト・六水和物(純度99.5%)1.19g(5ミリモル)、和光純薬工業(株)製の塩化第一鉄・四水和物(純度99.9%)0.509g(2.5ミリモル)および脱イオン水1000cm3を入れた。フラスコの中に窒素ガスを一晩流し続けることにより、フラスコ中の空気を窒素ガスで置換した。該フラスコの中に、和光純薬工業(株)製のヘキサメチレンテトラミン(純度99.0%)21.0gを入れ、引き続き、窒素ガスを流すと共に、内容物を撹拌しながら、5時間還流した。沈殿したピンク色の固体を窒素ガスで満たした装置の中でろ過し、脱イオン水で3回、無水エタノールで2回洗浄した。収量はおよそ0.5gであった。
なお、すでに述べたことであるが、念のため実施例においても再説すれば、ここで使用するクロロホルムには、ごく少量(およそ30ppm)の水が含まれていたほうが目的生成物を得るのに都合がよい。つまり、完全に無水のクロロホルムを使用した場合に酸化が不完全であったことや無水のクロロホルムに少量の水を添加するとよい結果が得られたことから、水酸化コバルト(II)・鉄(II)層状結晶から水酸化コバルト(II)・鉄(III)六角板状層状結晶に変換させるには少量の水の存在が不可欠であることが分かった。
和光純薬工業(株)製の過塩素酸ナトリウム・一水和物(純度98.0%)175gと和光純薬工業(株)製の濃度0.1モル/Lの塩酸水溶液5cm3に脱イオン水495cm3を加えた溶液を三角フラスコに入れ、さらに、実施例で製造されたCo0.67Fe0.33(OH)2I0.22(CO3)0.055・0.3H2O 0.5gを入れて分散させ、三角フラスコ内を窒素ガスで置換し、室温で1日間振盪させた。褐色の粉末をろ過し、水で洗浄した後、空気中で乾燥した。収量は0.44gであった。
Claims (5)
- 水酸化コバルト(II)・鉄(II)六角板状層状結晶をヨウ素及び水のクロロホルム溶液中で処理するステップを含む、ヨウ素アニオンがインターカレートされた水酸化コバルト(II)・鉄(III)六角板状層状結晶の製造方法。
- 前記処理するステップは、ヨウ素及び水のクロロホルム溶液中に水酸化コバルト(II)・鉄(II)六角板状層状結晶を分散させ、室温で攪拌するステップである、請求項1に記載のヨウ素アニオンがインターカレートされた水酸化コバルト(II)・鉄(III)六角板状層状結晶の製造方法。
- 前記水酸化コバルト(II)・鉄(II)六角板状層状結晶はブルーサイト型結晶である、請求項1または2に記載のヨウ素アニオンがインターカレートされた水酸化コバルト(II)・鉄(III)六角板状層状結晶の製造方法。
- 前記水酸化コバルト(II)・鉄(II)六角板状層状結晶は厚さが1×102nm〜5×102nmである、請求項1から3の何れかに記載のヨウ素アニオンがインターカレートされた水酸化コバルト(II)・鉄(III)六角板状層状結晶の製造方法。
- 前記水酸化コバルト(II)・鉄(II)六角板状層状結晶は、塩化コバルト・六水和物と塩化第一鉄・四水和物との混合物の水溶液に窒素ガスを流すと共にヘキサメチレンテトラミンを加えた後、還流させることにより製造される、請求項1〜4の何れかに記載のヨウ素アニオンがインターカレートされた水酸化コバルト(II)・鉄(III)六角板状層状結晶の製造方法。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012005050A JP5614689B2 (ja) | 2012-01-13 | 2012-01-13 | 水酸化コバルト(ii)・鉄(iii)六角板状層状結晶の製造方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2012005050A JP5614689B2 (ja) | 2012-01-13 | 2012-01-13 | 水酸化コバルト(ii)・鉄(iii)六角板状層状結晶の製造方法 |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2007138187A Division JP2008290913A (ja) | 2007-05-24 | 2007-05-24 | 水酸化コバルト・鉄結晶および水酸化コバルト・鉄単層ナノシートならびにそれらの製造方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2012076996A JP2012076996A (ja) | 2012-04-19 |
JP5614689B2 true JP5614689B2 (ja) | 2014-10-29 |
Family
ID=46237656
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2012005050A Expired - Fee Related JP5614689B2 (ja) | 2012-01-13 | 2012-01-13 | 水酸化コバルト(ii)・鉄(iii)六角板状層状結晶の製造方法 |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP5614689B2 (ja) |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20050260271A1 (en) * | 2004-05-20 | 2005-11-24 | Eastman Kodak Company | Composition comprising layered host material with intercalated functional-active organic compound |
JP2005335965A (ja) * | 2004-05-24 | 2005-12-08 | National Institute For Materials Science | ヘキサメチレンテトラミンを用いた均一沈殿法による良質な層状複水酸化物の製造方法およびその用途 |
JP5187797B2 (ja) * | 2005-07-25 | 2013-04-24 | 独立行政法人物質・材料研究機構 | 層状複水酸化物を剥離する方法、複水酸化物ナノシート、該複合薄膜材料、該製造方法、および、層状複水酸化物薄膜材料の製造方法 |
-
2012
- 2012-01-13 JP JP2012005050A patent/JP5614689B2/ja not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JP2012076996A (ja) | 2012-04-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Wu et al. | Single-crystalline α-Fe 2 O 3 nanostructures: controlled synthesis and high-index plane-enhanced photodegradation by visible light | |
Thirumalairajan et al. | Photocatalytic degradation of organic dyes under visible light irradiation by floral-like LaFeO 3 nanostructures comprised of nanosheet petals | |
Zhang et al. | Retracted Article: Formation of Fe 3 O 4@ MnO 2 ball-in-ball hollow spheres as a high performance catalyst with enhanced catalytic performances | |
Wang et al. | Morphology and composition controllable synthesis of Mg–Al–CO3 hydrotalcites by tuning the synthesis pH and the CO2 capture capacity | |
Cai et al. | Template-free synthesis of hierarchical spindle-like γ-Al 2 O 3 materials and their adsorption affinity towards organic and inorganic pollutants in water | |
Wang et al. | Single-crystalline ZnSn (OH) 6 hollow cubes via self-templated synthesis at room temperature and their photocatalytic properties | |
Dong et al. | Single-crystalline mesoporous ZnO nanosheets prepared with a green antisolvent method exhibiting excellent photocatalytic efficiencies | |
Wang et al. | Metal oxide decorated layered silicate magadiite for enhanced properties: insight from ZnO and CuO decoration | |
Xie et al. | Template-free synthesis of zinc citrate yolk–shell microspheres and their transformation to ZnO yolk–shell nanospheres | |
Jiang et al. | Potassium niobate nanostructures: controllable morphology, growth mechanism, and photocatalytic activity | |
Qin et al. | Synthesis of Au and Au–CuO cubic microcages via an in situ sacrificial template approach | |
Sun et al. | Facile synthesis of porous Bi 2 WO 6 nanosheets with high photocatalytic performance | |
Yang et al. | Control of the formation of rod-like ZnO mesocrystals and their photocatalytic properties | |
Tong et al. | High-quality elliptical iron glycolate nanosheets: selective synthesis and chemical conversion into Fe x O y nanorings, porous nanosheets, and nanochains with enhanced visible-light photocatalytic activity | |
JP5910887B2 (ja) | 水膨潤性層状複水酸化物とその製造方法、ゲル状又はゾル状物質及び、複水酸化物ナノシートとその製造方法 | |
Peng et al. | Controllable synthesis and photoreduction performance towards Cr (vi) of BiOCl microrods with exposed (110) crystal facets | |
Jiang et al. | Fabrication of a novel graphene oxide/β-FeOOH composite and its adsorption behavior for copper ions from aqueous solution | |
Zhang et al. | MnO x-modified ZnAl-LDOs as high-performance adsorbent for the removal of methyl orange | |
Jung et al. | 3-D self-assembly of flower-like particles via microwave irradiation for water treatment | |
JP2008290913A (ja) | 水酸化コバルト・鉄結晶および水酸化コバルト・鉄単層ナノシートならびにそれらの製造方法 | |
JP6099040B2 (ja) | 複合化層状複水酸化物 | |
Abdelbasir et al. | Controlling the optical and magnetic properties of nanostructured cuprous oxide synthesized from waste electric cables | |
Zhou et al. | Synthesis and catalytic property of facet-controlled Co 3 O 4 structures enclosed by (111) and (113) facets | |
Davar et al. | Synthesis and characterization of cobalt oxide nanocomposite based on the Co3O4–zeolite Y | |
Pudukudy et al. | Facile chemical synthesis of nanosheets self-assembled hierarchical H2WO4 microspheres and their morphology-controlled thermal decomposition into WO3 microspheres |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20120116 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20120127 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20120525 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20131203 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20140128 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20140401 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20140819 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20140829 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 5614689 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
LAPS | Cancellation because of no payment of annual fees |